Methanol → Methyl 4-Iodo-3-methylbenzoate
反応式
[CH3:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[I:11])[C:5]([OH:7])=[O:6].S(=O)(=O)(O)O.[CH3:17]O>>[CH3:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[I:11])[C:5]([O:7][CH3:17])=[O:6]参加物
4
実験手順
24.4 g (0.093 mol) of 3-methyl-4-iodobenzoic acid and 250 ml of methanol were introduced into a round-bottomed flask and 2.5 ml of concentrated sulfuric acid were added dropwise. Heating was carried out at reflux for twelve hours, the reaction mixture was evaporated and the residue taken up in ethyl acetate and water. The organic phase was separated by settling, dried over magnesium sulfate and evaporated. The residue was triturated in methanol and filtered. 21.9 g (85%) of the expected methyl ester, with a melting point of 58°-59° C., were recovered.
後処理
- temperatureHeating
- temperatureat reflux for twelve hours
- customthe reaction mixture was evaporated
- customThe organic phase was separated
- dry with materialdried over magnesium sulfate
- customevaporated
- customThe residue was triturated in methanol
- filtrationfiltered
- custom21.9 g (85%) of the expected methyl ester, with a melting point of 58°-59° C., were recovered
出典と根拠
- ORDレコード
- ord-28e714b4d999404bbb4c92a95d3104a7
- 出典データセット
- uspto-grants-2002_04
- 特許番号
- US06368608B1
反応ノート
読み込み中…